CN114217012A - Method for in-situ modification of mercury quantum dots in traditional heat injection process - Google Patents

Method for in-situ modification of mercury quantum dots in traditional heat injection process Download PDF

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CN114217012A
CN114217012A CN202111324623.0A CN202111324623A CN114217012A CN 114217012 A CN114217012 A CN 114217012A CN 202111324623 A CN202111324623 A CN 202111324623A CN 114217012 A CN114217012 A CN 114217012A
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CN114217012B (en
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刘晶晶
王建禄
郭天乐
黄新宁
孟祥建
沈宏
林铁
褚君浩
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Shanghai Institute of Technical Physics of CAS
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Abstract

The invention belongs to the field of compound semiconductor nano material preparation, and particularly discloses an in-situ modification method for mercury quantum dots in a traditional heat injection process. The method is characterized in that: in the traditional process of synthesizing HgTe quantum dots by hot injection, after reaction for a certain time, two-phase liquid level separation occurs in the mixed reaction by quickly injecting low-boiling-point polar liquid which is mutually incompatible with a reaction solvent, and selective crystal orientation surface modification is carried out on the surfaces of mercury quantum dots. Taking HgTe quantum dots with a medium-wave infrared (3-10 microns) cut-off wavelength as an example, after the in-situ modification, the quantum dots are close to spherical in appearance and good in symmetry, the monodispersity and size uniformity of the quantum dots are improved, and the quantum dots have good electrical characteristics and enhanced photoelectric detection performance.

Description

Method for in-situ modification of mercury quantum dots in traditional heat injection process
The technical field is as follows:
the invention belongs to the field of compound semiconductor nano material preparation, and particularly discloses an in-situ modification method for mercury quantum dots in a traditional heat injection process.
Background art:
in the last two decades, with the rapid development of nanotechnology and material science, hundreds of low-dimensional novel semiconductor materials are emerged. Due to the unique three-dimensional quantum confinement effect of the quantum dot material, the direct energy band gap can be adjusted through size control, peculiar characteristics are possessed on a plurality of physical properties such as light, electricity and magnetism, and great application potential is shown in the fields of photoelectronic devices and the like. In the medium wave infrared region, due to the special negative band gap structure in the mercury telluride (HgTe) bulk material, the response wave band of the corresponding quantum dot can be adjusted from near infrared to terahertz, and the material has wide commercial and military application values.
The excellent application potential of the mercury telluride quantum dot puts high requirements on the synthesis and preparation quality of the mercury telluride quantum dot, and particularly in the fields such as infrared photoelectric detection and the like related to military application, the rigorous requirements on the performance of the mercury telluride quantum dot need the quantum dot with extremely high quality, such as the characteristics of uniform height and size, extremely low surface defect, high carrier mobility and the like. At present, mercury telluride quantum dots synthesized by a colloidal chemical method based on solution operation have not been reported to have uniform dimension height, such as HgTe and HgSe colloidal quantum dots reported in Nature Communications,2019,10:2125, J.Phys.chem.C 2020,124,29, 16216-. Meanwhile, the surface morphology of the quantum dots is mainly triangular polygon, which is not beneficial to long-range ordered close packing, and finally reduces the key performance of the quantum dot device, such as mobility, responsivity and the like.
The invention content is as follows:
the invention mainly aims to solve the problems of irregular appearance and large size deviation of the conventional mercury-system quantum dot heat injection synthetic sample, and provides an in-situ modification method for the mercury-system quantum dot in the traditional heat injection process. In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
providing initial non-spherical HgTe quantum dots;
in the initial HgTe quantum dot synthesis process, a low-boiling-point polar solvent which is immiscible with a reaction solvent is injected into a mixed reaction system containing trimethylsilyl tellurium, amine and a mercury source after a certain time, and selective crystal orientation surface modification is carried out on the surface of the HgTe quantum dot.
In some preferred embodiments, the injection time and conditions of the polar solvent include: reacting a mixed reaction system containing trimethylsilyl tellurium, amine and a mercury source at 80-120 ℃ for 1-20 min; injecting a polar solvent after 1-20 min of the mixing reaction, and continuing the reaction for 10-60 min.
Further, the post-injected polar solvent includes any one or a combination of two or more of methanol, acetonitrile, water, acetone, chloroform, and isopropanol, and preferably methanol, but is not limited thereto.
The embodiment of the invention also provides the quantum dot synthesized by the method.
Furthermore, the size of the quantum dots is 6-13 nm, the size distribution square mean deviation is less than 10%, the absorption cut-off wavelength is 3-10 microns, and the wavelength is adjustable in a medium-wave infrared spectrum.
Compared with the prior art, in the growth process of the HgTe quantum dot, the two-phase liquid level mixing in the reaction is realized by using the polar solvent injected by the method, and the evaporation of the low-boiling point injected solvent is adopted to carry out surface directional modification while growing, so that the accumulation of excessive trimethylsilyl tellurium on the surface of the quantum dot along a specific crystal direction can be avoided, the regularity of the quantum dot is improved, the surface defect is reduced, and the quantum efficiency is improved. In addition, due to surface modification, the quantum dot product has good monodispersity, highly uniform size and high film mobility.
Description of the drawings:
fig. 1 is a flow chart of an in-situ modification method in a traditional thermal injection process of mercury quantum dots.
FIG. 2 is a comparison graph of the absorption spectra of HgTe quantum dots with polar solvent added in the reaction and the original HgTe quantum dots.
FIG. 3 is a Transmission Electron Microscope (TEM) and a statistical comparison of the HgTe quantum dots with the original HgTe quantum dots added with the polar solvent in the reaction according to the present invention.
FIG. 4 is an X-ray diffraction spectrum of HgTe quantum dots with polar solvent added in the reaction according to the present invention.
Fig. 5 is a graph comparing the electrical properties of the HgTe quantum dots with the original HgTe quantum dots added with a polar solvent in the reaction according to the present invention.
The specific implementation mode is as follows:
in order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A HgTe quantum dot preparation process and an in-situ modification method based on thermal injection comprise the following steps:
raw materials:
mercuric chloride (HgCl)2) Sigma-Aldrich 99.5％
Oleamine Oleyamine (OAm) Aladdin 80-90%
Trimethylsilyl Tellurium (TMS)2Te) Sigma-Aldrich 99.5％
The first step is as follows: putting the raw materials into a 100ml three-neck flask, vacuumizing, heating to 80 ℃ until no bubbles exist, heating to the reaction temperature of 100 ℃, fully dissolving mercury chloride, and then opening an argon valve to open the flask, wherein the flask is in an argon environment.
The second step is that: and (3) reheating the prepared oleylamine mercuric chloride solution to the reaction temperature of 100 ℃, quickly injecting trimethylsilyl tellurium diluted in a normal hexane solvent in an argon environment, and reacting for 3 minutes.
The third step: further, after the above mixed system was reacted for 1 minute, a low-boiling polar solvent was rapidly injected and stirred.
The fourth step: and (3) injecting the solution after the reaction in the third step into 8ml of TCE solution to further terminate the reaction, and cooling the mixed solution to 0 ℃ in an ice-water mixed solution.
The fifth step: adding the reaction solution in the fourth step in a volume ratio of 1: 2-1: 10 of absolute ethyl alcohol at 10000rpm for 5 minutes, and after centrifugation, the supernatant is discarded. And obtaining the modified high-quality HgTe quantum dot solution.
Example 2
The preparation process of the HgTe quantum dot with the diameter of 6.5 nanometers comprises the following steps:
all the steps are the same as example 1, and HgTe quantum dots with the cut-off wavelength of 6.5 nm can be obtained only by changing the reaction temperature in the second step to 90 ℃.
Example 3
The preparation process of HgTe quantum dots with the diameter of 13 nanometers comprises the following steps:
all the steps are the same as example 1, and HgTe quantum dots with a diameter of 13nm can be obtained only by changing the reaction temperature in the second step to 110 ℃.
Comparative example 1
All steps are the same as in example 1, except that the rapid injection of the polar solvent in the third step is removed.
The quantum dots obtained in example 1 and comparative example 1 were characterized:
the optical absorption characteristics of a film with the thickness of about 500 nanometers prepared by dripping and coating a quantum dot solution are measured on a Fourier spectrometer, and the absorption spectrum is shown in figure 2, so that the quantum dots prepared in the embodiment 1 have more fine structures visible at room temperature and have more regular morphology and size distribution.
The quantum dot solution is dropped on an ultrathin carbon film copper net, naturally dried and imaged under a high-resolution Transmission Electron Microscope (TEM), as shown in FIG. 3, it can be seen that the quantum dot monodispersion degree of the example 1 is high, and the size distribution square mean deviation is significantly smaller than that of the comparative example 1.
The diffraction pattern of the quantum dots is measured on an X-ray diffractometer, and as shown in FIG. 4, the mercury telluride HgTe quantum dots successfully prepared in example 1 can be obtained through analysis and comparison.
Example 4:
preparing a light guide type detector with a cut-off wavelength of 5 microns HgTe quantum dot horizontal structure:
substrate selection: heavily doped p-type silicon with the thickness of 0.5 mm is selected as a substrate.
Preparing an oxide dielectric layer: and oxidizing the surface of the silicon substrate by a thermal oxidation method to prepare silicon dioxide with the thickness of 285 +/-5 nanometers.
Preparing a source electrode and a drain electrode: preparing interdigital electrode patterns of a source electrode and a drain electrode by using an electron beam lithography method; preparing a metal electrode by utilizing a thermal evaporation technology, wherein the chromium is 10 nanometers, and the gold is 20 nanometers; and stripping the metal film by combining a stripping method to obtain a source electrode and a drain electrode, wherein the width of a channel is 10 microns.
Preparing a quantum dot working film: the quantum dot solution prepared in example 1 was spin-coated on the prepared interdigitated electrode. After the solvent is naturally volatilized, ligand exchange is carried out through 2% of 1, 2-ethanedithiol by volume percentage, and long-chain oleylamine wrapped outside the quantum dots is replaced. And repeating the processes of spin coating and ligand replacement until the thickness of the quantum dot working film reaches 100-1000nm, wherein the thickness is preferably 100 nm.
Electrical testing of quantum dot thin film devices:
and applying a bias voltage of a tiny constant 0.1V between the source electrode and the drain electrode, and detecting the channel current of the HgTe quantum dots, wherein the scanning range of the gate voltage is-40V to 40V, and the scanning direction of the gate voltage is from negative to positive to negative. Measuring the transfer characteristic of the device under the dark and non-illumination condition of a temperature-changing probe station, wherein the electron mobility tested by a field effect transistor is shown in fig. 4, and the mobility of example 1 is much higher than that of comparative example 1 and exceeds nearly 2 orders of magnitude; in addition, dark current level example 1 is lower than comparative example 1 due to fewer defects in the film.
Photoelectric test of quantum dot thin film device:
applying a bias voltage of a tiny constant 0.1V between a source electrode and a drain electrode, detecting the channel current of a device of HgTe quantum dots radiated by a 600K blackbody light source under the modulation of a chopper, reading the signal through a preamplifier (SR570) and a lock-in amplifier (SR830), and obtaining the normalized detection rate of 1 multiplied by 10 under the room-temperature working condition8Jones。
In conclusion, by the technical scheme, the invention can realize more uniform growth of HgTe quantum dots, and the obtained quantum dot product has high uniformity in size and good monodispersity.
In addition, the present inventors have also conducted experiments under the conditions and the like listed in the present specification with reference to the manner of examples 1 to 3, and produced highly uniform monodisperse HgTe quantum dots of different cutoff wavelengths.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. For example, parts not described in the present specification may be implemented by taking or referring to the prior art, and therefore, all equivalent changes or modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (4)

1. A method for in-situ modification of mercury quantum dots in a traditional heat injection process is characterized by comprising the following steps:
the first step is as follows: preparing a precursor solution: mixing halide of mercury and amine solvent, heating to 100 ℃, and fully stirring to form a precursor of mercury;
the second step is that: and (2) quickly injecting the trimethylsilyl tellurium into a mixed reaction system of a mercury precursor and an amine solvent at the reaction temperature of 80-120 ℃. Preferably, the molar ratio of tellurium to mercury to oleylamine is 0.5:1: 48;
the third step: in the process of mixing reaction, injecting a certain amount of polar solvent, and carrying out in-situ surface modification on the quantum dots in a two-phase dynamic interface;
the fourth step: and cooling, separating and purifying to obtain the medium-wave infrared mercury quantum dot solution.
2. The method for in-situ modification in traditional thermal injection process of mercury-based quantum dots according to claim 1, wherein the halide of mercury in the first step is one or more of mercuric chloride, mercuric bromide and mercuric iodide mixed in any proportion, and the molar concentration of mercury is 0.03-0.1 mol/L.
3. The method according to claim 1, wherein the amine solvent in the first and second steps comprises any one or a combination of two or more of oleylamine, octadecylamine, hexadecylamine, tetradecylamine, dodecylamine, n-octylamine, and trioctylamine.
4. The method of claim 1, wherein the polar solvent in the third step comprises one or more of methanol, acetonitrile, water, acetone, chloroform, and isopropanol, and the volume ratio of the polar solvent to the amine solvent in the second step is 1: 4.
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